Complexes [PPN][NiIII(OR)(P(C6H3-3-SiMe3-2-S)3)] (R = OPh (1), OMe (3)),
obtaining from reactions of complexes [PPN][NiIII(Cl)(P(C6H3-3-SiMe3-2-S)3)] and 1
with 3 equiv of [Na][OPh] and 1 equiv of [n-Bu4N][OMe] in THF-MeCN and
THF-MeOH, respectively, are good precursors to synthesize the other NiIII complexes
[PPN][NiIII(L)(P(C6H3-3-SiMe3-2-S)3)] (L = SPh (2), StBu (4), S(CH2)2SH (5),
SC6H4-o-OH (6), SSSMe (7), SeSeMe (8), CCPh (9)), characterized by UV-vis,
electron paramagnetic resonance (EPR), cyclic voltammetry (CV), and single-crystal
X-ray diffraction.
Complex 3 triggers coordination and activation of CO2 to yield the thermally
stable complex [PPN][Ni(κ1-OCO)(P(C6H3-3-SiMe3-2-S)3)] (10), upon CO2 bubbled
into the THF solution of complex 3 at ambient temperature. The electronic structure
of complex 3 was identified as a separated system of NiIII and OCO radical,
characterized by X-ray absorption and EPR spectra. Reactions of complex 10 and
[PPN][NiIII(NCO)(P(C6H3-3-SiMe3-2-S)3)] (11) with TMSCl producing free CO2 and
TMS-NCO, respectively, identified the cores of M-OCO and M-NCO. In addition,
reaction of complex 10 and 11 with excess CS2, produce complexes
[PPN][NiIII(NCS)(P(C6H3-3-SiMe3-2-S)3)] (13) and [PPN][Ni(OCS)(P(C6H3-3-
SiMe3-2-S)3)] (14), respectively, an unprecedented metal-complex containing κ1-OCS
ligand.
Complex [PPN][NiIII(NO2)P(C6H3-3-SiMe3-2-SH)3] (15), synthesized from NO
gas purging into THF solution of complex 3 via the mechanism of NO
disproportionation reaction, could activate S8 to lead to the known bridging complex
[PPN]2[(NiIII(P(C6H3-3-SiMe3-2-SH)3))2(S8)] by the pathway 2NO2－ + S8 → 2NO2 + S82－.

錯合物[PPN][NiIII(Cl)(P(C6H3-3-SiMe3-2-S)3)] 與[PPN][NiIII(OPh)(P(C6H3-3-
SiMe3-2-S)3)] (1) 分別加入三當量的[Na][OPh] 及一當量的[n-Bu4N][OMe] 在
THF-MeCN 及THF-MeOH 混合溶液中反應， 依序可得到錯合物1 及
[PPN][NiIII(OMe)(P(C6H3-3-SiMe3-2-S)3)] (3)。此兩以氧為配位基的錯合物為有效
的前驅物，可進而合成其他鎳三價錯合物[PPN][NiIII(L)(P(C6H3-3-SiMe3-2-S)3)] (L
= SPh (2), StBu (4), S(CH2)2SH (5), SC6H4-o-OH (6), SSSMe (7), SeSeMe (8), CCPh
(9))，並且以多種光譜技術(紫外-可見光光譜、電子順磁共振光譜及單晶X 光繞
射分析)及循環伏安法鑑定之。
在室溫下，將二氧化碳導入溶有錯合物3 的THF 溶液中，錯合物3 能引發
二氧化碳配位在鎳金屬上且活化之，進而得到一熱穩定的錯合物[PPN][Ni-
(κ1-OCO)(P(C6H3-3-SiMe3-2-S)3)] (10)。藉由X 光吸收光譜及電子順磁共振光譜的
分析，錯合物10 為一鎳三價中心配位著被還原的二氧化碳自由基陰離子(carbon
dioxide radical anion)。錯合物10 及[PPN][NiIII(NCO)(P(C6H3-3-SiMe3-2-S)3)] (11)
可與三甲基氯矽烷(TMSCl)反應，分別釋放出二氧化碳及異氰酸三甲基矽酯
(TMS-NCO)，由此可以區別出金屬離子配位著二氧化碳及異氰酸根兩者的不同
之處。此外，過量的二硫化碳可將錯合物10 及11 分別轉換成錯合物
[PPN][NiIII(NCS)(P(C6H3-3-SiMe3-2-S)3)] (13) and [PPN][Ni(OCS)(P(C6H3-3-
SiMe3-2-S)3)] (14)。其中，氧硫化碳(OCS)以立接模式(end-on)配位在鎳離子上的
錯合物14 為一新發現。
過量的一氧化氮氣體通入溶有錯合物3 的THF 溶液，經自身氧化還原反應
可得到具有亞硝酸根配位的錯合物[PPN][NiIII(NO2)P(C6H3-3-SiMe3-2-SH)3]
(15)。錯合物15 可與硫粉反應生成已知的帶負二價之八硫鍊雙核錯合物
[PPN]2[(NiIII(P(C6H3-3-SiMe3-2-SH)3))2(S8)]，推測其反應機構為三價鎳氧化亞硝
酸根獲得電子進而還原硫粉。

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